高等离子体功率密度下MPCVD法制备多晶金刚石膜

何中文; 马志斌

doi:10.13394/J.cnki.jgszz.2021.0121

高等离子体功率密度下MPCVD法制备多晶金刚石膜

doi: 10.13394/J.cnki.jgszz.2021.0121

何中文,
马志斌^,

武汉工程大学材料科学与工程学院, 等离子体化学与新材料湖北省重点试验室, 武汉 430073

详细信息

通讯作者:
马志斌，男，1968年生，教授、博导。主要研究方向：等离子体技术与CVD金刚石。E-mail: mazb@wit.edu.cn

中图分类号: TQ164
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出版历程
- 收稿日期: 2021-07-11
- 修回日期: 2021-12-27
- 录用日期: 2022-03-18
- 刊出日期: 2022-05-27

Preparation of polycrystalline diamond films by MPCVD at high plasma power density

HE Zhongwen,
MA Zhibin^,

Key Laboratory of Plasma Chemical and Advance Materials of Hubei Province, School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan 430073, China

摘要

摘要: 通过自制的MPCVD双基片台设备，在微波功率为1400 W保持不变及中高气压，等离子体功率密度为357.5～807.4 W/cm³，基片温度为850 ± 30 ℃，CH₄体积分数为1.0%～1.5%，沉积速率为1～8 μm/h条件下，在直径11.5 mm的硅基片上沉积不同质量的多晶金刚石膜，并通过光谱仪、光学显微镜、拉曼光谱仪对等离子体中的氢原子及含碳基团、多晶薄膜的形貌及质量进行表征。结果表明：随着等离子体功率密度上升，等离子体椭球中的氢原子基团和含C的活性基团强度增加，金刚石膜生长速率大幅度提高，金刚石膜纯度也大幅度提升。在气压为21 kPa，等离子体功率密度为807.4 W/cm³，基片温度为850±30 ℃，生长时间为150 h，CH₄体积分数为1.0%及氢气流量为200 mL/min的条件下，金刚石膜的生长速率达到5 μm/h，金刚石膜厚达752.0 μm，金刚石拉曼峰的半高宽为6.48 cm⁻¹，且生长的金刚石膜质量良好。
- 微波等离子体化学气相沉积 /
- 金刚石膜 /
- 等离子体功率密度 /
- 沉积速率 /
- 薄膜质量
Abstract: Through the self-made MPCVD dual-substrate platform equipment, the microwave power was 1 400 W and the pressure was medium to high, the plasma power density was 357.5～807.4 W/cm³, the substrate temperature was 850 ± 30 ℃, the volume fraction of CH₄ was 1.0%～1.5% and the deposition rate was 1～8 μm/h, the polycrystalline diamond film of different quality was deposited on the silicon substrate with a diameter of 11.5 mm. The hydrogen atoms and the C-containing groups in the plasma, the morphology and the quality of polycrystalline films were characterized by spectrometer, optical microscope and Raman spectrometer. The results show that with the increases of plasma power density, the strength of hydrogen atom group and active C-containing group in plasma ellipsoid increase, the growth rate and the purity of diamond film are greatly improved. When the air pressure is 21 kPa, the plasma power density is 807.4 W/cm³, the substrate temperature is 850 ± 30 ℃, the growth time is 150 h, the CH₄ volume fraction is 1.0% and the hydrogen flow rate is 200 mL/min, the growth rate of the diamond film reaches 5 μm/h, the thickness of the diamond film reaches 752.0 μm, the FWHM of the diamond Raman peak is 6.48 cm⁻¹, and the quality of the grown diamond film is good.
- microwave plasma chemical vapor deposition (MPCVD) /
- diamond film /
- plasma power density /
- deposition speed /
- film quality

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图 1 双基片结构中的等离子体球形状

Figure 1. Plasma sphere shape in double substrate structure

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图 2 条件8#时的等离子体发射光谱图

Figure 2. Plasma emission spectrum under condition 8#

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图 3 中高气压下H_β和C₂基团的谱线强度随功率密度的变化

Figure 3. Variation of spectral line intensities of H_β and C₂ group with power densities at medium and high pressures

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图 4 1#～6#金刚石膜生长速率随等离子体功率密度的变化

Figure 4. Variation of 1#～6# diamond film growth rates with plasma power densities

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图 5 样品表面的SEM形貌

Figure 5. SEM morphologies of sample surface

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图 6 4个样品的Raman光谱图

Figure 6. Raman spectra of four samples

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表 1 金刚石膜生长参数

Table 1. Diamond film growth parameters

条件及编号	气压 p / kPa	等离子体功率密度 η / (W·cm⁻³)	基片温度 θ / ℃	生长时间 t / h	CH₄体积分数 φ / %	H₂流量 q_v / (mL·min⁻¹)	金刚石膜厚度 L / μm
1#	15	357.5	850±30	24	1.5	200	26.0
2#	16	416.7		72	1.5		158.4
3#	18	527.5		16	1.5		48.0
4#	19	596.7		36	1.5		144.0
5#	20	686.8		170	1.5		1 020.0
6#	21			100	1.5		801.0
7#		807.4		50	1.2		302.0
8#				150	1.0		752.0

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表 2 1#～8# 样品的拉曼峰半高宽

Table 2. FWHM of Raman peak of 1#～8# sample

样品	拉曼峰半高宽 d / （cm⁻¹）
1#	11.64
2#	7.94
3#	7.90
4#	7.58
5#	7.79
6#	6.87
7#	6.74
8#	6.48

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参考文献(13)

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